反応 #63494

反応方程式

ammonia

3-(2,3β-dihydro-6-methyl-12-nitro-8α-ergolinyl)-1,1-diethylurea

sodium borohydride

hydrochloric acid

→

3-(12-amino-2,3-dihydro-6-methyl-8α-ergolinyl)-1,1-diethylurea

収率 97.9%

溶媒

methanol

反応条件

後処理

1. 1
   温度cooled in an ice bath
2. 2
   抽出extracted
3. 3
   その他After drying
4. 4
   その他evaporation of the organic phase

実験手順

One millimole of 3-(2,3β-dihydro-6-methyl-12-nitro-8α-ergolinyl)-1,1-diethylurea is dissolved in 25 ml of methanol, cooled in an ice bath, and 2 mmol of nickel chloride (with 6H2O) and thereafter 5 mmol of sodium borohydride are added thereto in 4-5 portions. Under ice cooling, the mixture is acidified with 2N hydrochloric acid, combined with dilute ammonia solution, and extracted by shaking. After drying and evaporation of the organic phase, 350 mg of 3-(12-amino-2,3-dihydro-6-methyl-8α-ergolinyl)-1,1-diethylurea is obtained. [α]D =-31° (0.5% methanol) as the tartaric acid salt (1:1).

出典